Apparatus for obtaining absolute alcohol



June 1 i926. 3,586,711

J. A. STEFFENS APPARATUS FOR OBTAINING ABSOLUTE ALCOHOL Filed April 5,1921 Patented June 1 1926.

1,586,718 PATENT OFFICE.

JOHN A. STEFFENS, OF BALTIMORE, MAR YLAND, ASSIGNOR TO U. S. INDUSTRIALALCOHOL 00., A CORPORATION OF WEST VIRGINIA.

APPARATUS FOR OBTAINING ABSOLUTE ALCOHOL.

Application filed April 5, 1921. Serial No. 458,884.

an apparatus whereby alcohols may be sep-' arated from water andespecially "by means of which absolute alcohol may be obtained inaccordance with a commercially practicable system.

More particularly, the object of m :vention is to provide an apparatusinased upon the utilization of a third liquid which is miscible with thealcohol but substantially immiscible with water and which is of such acharacter that when the three constituents are present vapors of thesame are evolved by distillation containing a considerable percentage ofwater and the third liquid so that all the water and the third liquidmay be removed in this way from the residual constituent, which is thealcohol. The evolved vapors are comprised of a ternary mixture of threeconstituents. This third liquid may be of any one of a number ofdifi'erent compounds, such, for example, as benzol, carbontetrachloride, hexane, etc., but I prefer to use benzol.

One of the objects of my invention is to avoid the necessity of using alarge amount of benzol in carrying out the apparatus.

A further object is to so arrange the apparatus as to enable a closeregulation thereof to be obtained, inasmuch as in m appa ratus thedehydration of the alcoho is carried out in a column, the upper portionof i which is fed continually with a quantity of the condensate of.fixedcomposition passing out of the top of the tower, as a condensate rich inwater is obtained with a comparatively small load being placed upon theauxiliary apparatus and as the alcohol evolved in the form of vapor isreturned to the tower continually in the form of'a liquid having .afixed composition obtained by a uniform rectification of the recoveredalcohol.

Again, another object is to operate the apparatus so that a drier benzolis obtained owing to the separation of the condensate before introducingwater into the same.

A further object is to so arrange the sysv tem as to enable the severaloperations to be carried out continuously, but so that the severaloperations may be carried out large- 1y independently of the remainingoperations, thus enabling the operator of the system to recover in caseat any time any one of the operations does not function. This is broughtabout especially by reason of the com lete removal of the benzol fromthe disti late prior to the rectification of the dilute alcohol. Breason of these features 1n my apparatus t e system may be operatedcontinuously.

Further objects Will appear from the detsptled description thereofcontained hereina er.

IVhile my invention is capable. of embodiment in many different forms, Ihave shown only one form of the same in the accompanying drawings, inwhich- The figure is adia-grammatic representation of an apparatus madein accordance with my invention.

In the drawings, I have shown a valved inlet pipe 1 for feedingcontinuously into the apparatus an alcohol mixed with water, and which,by way of example, may feed to the system ethyl alcohol having astrength of 95%. Leading into the pipe 1 there is a valved supply pipe 2for supplying initially the desired quantity of the third liquid, as,for example, benzol, and for supplying to the system additional amountsof benzol to replace the small quantities thereof which are lost byevaporation therefrom. The'alcohol and benzol are fed to the system inportions such that in the circulating system, at any given time, therewould be approximately equal parts by weights of 95% alcohol and benzolbutpreferably a slightly smaller quantity of the benzol than of the 95%alcohol. The valved pipe 1 leads into a tail-box 3 which is connected bya, liquid sealed pipe 4 to a dehydrating column 5 which is constructedin any suitable manner but which may have, for example, a plurality ofplates the same as in the case of the usual alcohol rectifying column.The column 5 has at the bottom an inlet 6 and an outlet 6 for steam forheating the column indirectly. Vapors are evolved from the columncomprisin approximately 74.1% by weight of benzol, .4% by weight ofwater, and 18.5% by weight of alcohol and absolute alcohol flows fromthe liquid sealed outlet pipe 7. The evolved vapors, pass out by meansof a pipe 8 into a dephlegmator 9 which is connected by a liquidsealed-pipe 10 to the top plate of the column. The de-. phlegmator iscooled in the usual way with I the aid of water inlet and outlet pipes11 and 12. The uncondensed vapors from the dephlegmator 9 pass into acondenser through a pipe-13, the temperature in which is atapproximately 649 C.,.said condenser being cooled bv water passingthrough inletand outlet pipes 14 and 15 and the condensate therefromenters a vented sight-glass 16 from which a portion of the condensatepasses through a valved pipe 17 to the pipe 10 and thence to the top ofthe column 5.

- The main portion of the condensate is conducted by aipipe 18 to atail-box 19 and thence by a pipe 20 to a separating chamber Thecomposition of the respective layers is approximately as follows: Theupper layer contains approximately 85.6% by weight of benzol, 2.8% byweight of water, and 11.6% by weight of alcohol, while the lower layercontains approximately 8.1% by Weight of benzol, 40.6%v by weight ofwater and 51.3% by weight of alcohol. The upper layer is conveyed by avented pipe 22 having a liquid seal 23 back to the tower 5 "while thelower layer passes by a vented pipe 24 to a scrubber 25. In order toremove the remainder of the benzol, water is introduced into thescrubber 25' by a pipe 26 ,thus producing therein twolayers of liquid,the upper layer of which contains the remalnder of the henzol. Thebenzol layer is conducted from the scrubber b a vented ipe 27 to'theliquid seal 23 an thence to t e tower 5, while the lower layer isconveyed through avented liquid sealed pipe 28 to an alcohol rectifyingcolumn 29 having a steam inlet ipe 30 and an outlet 30" in the usual wayor indirect heating and a 1i uid sealed drawoif pipe 31 for water at thettom of the column. The lower portion of the column .29 is maintained ata temperature of just above 100 C.' The evolved alcohol vaporscontaining some water passout of the to of the column through a pipe 32to a dep legmator. 33, constructed an stantially the same as thedephlegmator 9and which is arranged to return the condensate therein tothe top of the column '29 by a liquid sealed pipe 34. The vapors'fromthe dephlegmator 33 pass through a pipe 35, the vapors in which are at atemperature. of

approximately 76 (1., to a condenser 36 con-- structed the same as thecondenser 13. The condensate from the condenser 36, which comprisesapproximately 95% alcohol enters a vented sight-glass 37 and a portionof the same passes back through a valved pipe 38 to the liquid sealed.pipe 34 and thence to portions thereof requiring observation are locatedupon an operating floor 41.

In carrying out my invention the alcohol containing water and the benzolis fed into the column 5, the lower portion of whichis maintained at atemperature slightly below 784 C. The vapors of alcohol, watcrand benzolwill be distilled from the top of the. column 5 thus leaving behindabsolute alcohol which passes out of the bottom of the column throughthe pipe 7. The evolved vapors pass into the dephlegmator 9, whencesomeof the condensate is returned to the. topmost plate in the column 5 andat thel same time a small portion of the condensate from the condenser13 is also conveyed into the tower at the same point, thus sealing theuppermost plates in the column with a liquid of a constant compositionand which is very close to the composition of the evolved vapors. Thisnot only provides uniform conditions at the top of the tower but enablesthe apparatus tobe conducted with a comparatively small quantity ofbenzol so that'the condensate reaching the separating chamber 21 will berich in the water to be removed. VVhen the liquid condensate reaches theseparating chamber 21- it immediately divides into two layers, the upperlayer, comprised principally of benzol, being conveyed backto the tower5, while the lower layer, comprised principally of alcohol and water but'containing some benzol, is conducted to the scrubber 25 where water isadded in the pro ortions of approximately one part by weight of water toone part by weight of the incoming liquid. This se arates out the benzolinto an upper layer w iich is conveyed back to the column 5, while thedilute alcohol is conducted to the alcohol rectifying column 29. Thiscolumn is required merely to rectify the alcohol, said column at itslower portion being maintainedat a temperature of a proximately 100 C.,thewater from whici passes out from the bottom of the column, while thealcohol, substantially 95% in strength, is collected as a condensatehaving a fixed composition and temperature, and as the benzol as beensubstantially entirely removed therefrom, the conditions in the upperportion of the column 5 are comparatively uniform so far as thecharacter of the incoming alcohol is concerned. Furthermore, inasmuch asthe bulk of the benzol is returned directly from the separatin chamber21 to would otherwise be the case and this also .conduces touniformityin the operation of the apparatus. For the same reason less water iscarried back into the column and there is consequently a more effectiveseparation of the alcohol from the water. By providing a system of thischaracter n which the several arts of the system operate without a greategree of dependence upon one another it is possible to conduct the aparatus with great uniformlty of resu tsand in such a way that thefailure of any portion of the system to function temporarily would notinterfere w th the effective operation of the system as a whole. Forthese reasons, furthermore, it is practlcable to obtain absolute alcoholwith a continuously operating apparatus.

While I have described my invention above in detail I wish it to beunderstood that man changes may be made thereln without ceparting fromthe spirit of the same.

By the term scrubber in the claims is meant a device for scrubbing theliquid from the separator so as to further separate the constituents byordinary scrubbing action.

I claim:

1. An apparatus comprising a rectifier, a condenser connected thereto, aseparating chamber connected to the condenser and a scrubber connectedto the separating chamber.

2. An apparatus comprising a rectifier, a condenser connected thereto, aseparating chamber connected to the condenser, a scrubber connected tothe separating chamber and means for conveying liquids from theseparating chamber and scrubber back to the rectifier.

3. An apparatus comprising a rectifier, a condenser connected thereto, aseparating chamber connected to the condenser, a scrubber connected tothe separating chamber, means for conveying liquids from the separatingchamber and scrubber back to the rectifier and .a second rectifierconnected to the scrubber.

4. An apparatus comprising a rectifier, a condenser connected thereto, aseparating chamber connected to the condenser, a scrubber connected tothe separating cham ber, means for conveying liquids from theseparating'chamber and scrubber back to the rectifier. a secondrectifier connected to the scrubber, a condenser for the secondrectifier, and means for conducting the condensate from the secondrectifier to the first rectifier.

5. An apparatus comprisinga rectifier, a condenser connected thereto, aseparating chamber connected to the condenser, a scrubber connected tosaid separating chamber and adapted to receive a condensate therefrom, asecond rectifier connected to said scrubber, a dephlegmator andcondenser connected to the second rectifier so as to return a part ofthe condensate from said dephlegmator and last mentioned condenser tothe top of-the second rectifier, and means for conveying the condensatefrom the sec- 0nd recti er to the first rectifier.

6. An apparatus com rising a rectifier, a dephlegmator and con enserconnected to the rectifier so as to return a portion of the condensateto the top of the rectifier, a separating chamber connected to saidcondenser and adapted to receive condensate therefrom, a scrubberconnected to --said separating chamber and adapted to receive condensatetherefrom, a second rectifier connected to said scrubber, a dephlegmatorand condenser connected to the second rectifier so as to return a partof the condensate to the top of the second rectifier and means forconveying the condensate from the second rectifier to the firstrectifier.

7. An apparatus comprising a rectifier, a condenser connected directlythereto, a separating chamber connected to the condenser, a returnconduit from the separating chamber to the rectifier, means connected tothe said chamber for further separating liquid obtained from saidchamber, a conduit from said means for returning separated liquid tosaid rectifier, a second rectifier connected to said means, a condenserconnected to the second rectifier, and a return conduit connecting thiscondenser to the first-named rectifier.

8. An apparatus comprising a rectifier provided with feed conduits. nearits top and heating meansat its bottom, a-condenser for. the rectifier,a separating chamber and means for conveying the condensate from thecondenser to the separating chamber, a second rectifier connected to theseparating chamber, a condenser for the second rectifier, and means forconveying the condensate from the second rectifier to the firstrectifier.

9.-An apparatus comprising 'a rectifier provided with feed conduits nearits top and heating means at its bottom, a condenser for the rectifier,a separating chamber and means for conveying condensate from thecondenser to the separating chamber, means connected to the chamber-forfurther separating liquid obtained from said chamber, a conduit fromsaid means for returning separated liquid to said rectifier, a secondrectifier connected to the separating chamber, a condenser for thesecond rectifier, and means for conveying the condensate from the secondrectifier to the first rectifier.

In testimony that I claim the foregoing, I have hereunto set my handthis 26th day of January, 1921.

JOHN A. STEFFENS.

Certificate of Correction.

It is hereb certified that in Letters Patent No. 1,586,718, granted June1, 1926,

to John A. tefiens, of Baltimore, Maryland, for an improvement inApparatus for Obtaining Absolute Alcohol, an error appears in theprinted specificationv requirlng correction as follows: Page 3, line 90,claim 7 strike out the word directly and insert the same to follow afterthe word connected in line 91; and. that the said Letters Patent shouldbe read with this correction therein that the same may conform to therecord of the case in the Patent Ofiioe.

Signed and sealed this 13th day of July, A. D. 1926.

[sun] M. J. MOORE,

Acting 00mmz'88i0ner of Patents.

